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In this study, high purity gamma-alumina nanopowders with crystalline structures have been prepared via a sol–gel process by waste metal aluminum, HCl, NaOH, Polyethylene glycol (PEG) and polyvinyl alcohol (PVA). Polyethylene glycol and polyvinyl alcohol have been used as stabilizing agents. The characterization of the samples has been performed utilizing XRD, FTIR, SEM, N2 adsorption/desorption techniques. Prepared samples of gamma-alumina at 800∘C with PEG has an average crystallite size of 2.58[Formula: see text]nm, average particle size of 21[Formula: see text]nm, specific surface area (SSA) of 65.55[Formula: see text]m2/g, and pore volume of [Formula: see text]0.06[Formula: see text]cm3/g. The average crystallite size of 3.07[Formula: see text]nm, average particle size of 31[Formula: see text]nm, specific surface area of 131.25[Formula: see text]m2/g, and pore volume of [Formula: see text]0.14[Formula: see text]cm3/g, were obtained using PVA surfactant.